CN104152718B - A kind of method of stanniferous iron tailings separated in synchronization tin and iron - Google Patents
A kind of method of stanniferous iron tailings separated in synchronization tin and iron Download PDFInfo
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- CN104152718B CN104152718B CN201410347393.3A CN201410347393A CN104152718B CN 104152718 B CN104152718 B CN 104152718B CN 201410347393 A CN201410347393 A CN 201410347393A CN 104152718 B CN104152718 B CN 104152718B
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Abstract
The invention discloses a kind of method of stanniferous iron tailings separated in synchronization tin and iron, the method be by stanniferous iron tailings raw material and be made up of by a certain percentage sodium sulfate, borax and SODLUM FULVATE composite additive mixing after, agglomeration, dry, carry out oxidizing roasting successively again, reducing roasting is separated with magnetic separation, obtain tin residual quantity lower than 0.08% iron ore concentrate and the grade rich tailing that is greater than 1%, the rate of recovery of iron reaches more than 80%, achieves the high efficiency separation of iron and tin in tin iron tailings; The method pollute little, cost is low, and achieves the degree of depth comprehensive utilization of stanniferous iron tailings resource, be specially adapted to process tin iron symbiotic relationship closely, adopt existing beneficiation method to be difficult to the stanniferous iron tailings resource of Separation and Recovery.
Description
Technical field
The present invention relates to the method for a kind of stanniferous iron tailings comprehensive utilization, particularly a kind ofly from stanniferous iron milltailings, adopt the initial oxidation roasting associating roasting method Separation of Tin of magnetizing roasting and the method for iron again, belong to mineral processing and nonferrous metallurgy field.
Background technology
The typical feature of Tin Resources of China is: mostly be and bury dark, that distribution is overlapping skarn type lode tin mineral deposit, and cassiterite and the gangue mineral such as silicon, calcium and various metals mineral paragenesis, association are tight, and difficulty and the cost of thus mining, ore dressing and smelting are high.Current domestic tin ore reserves are about 3,000,000 tons, and workable reserve is only about 1,500,000 tons.Due to the weakening of exploitation and geological work in recent years for a long time, in addition the random mining of on a small scale enterprise a few years ago, the technique of preparing level adopted is general not high, cause most tinnery reserved resources not enough, thus potential threat is caused to the superiority of China's tin resource, had a strong impact on the healthy and sustainable development of domestic tin industry.With the situation of the producing level of current China tin resource, output and consumption, Tin Resources ensures that the time limit was less than 20 years.
Along with rising steadily of the day by day exhausted of Tin Resources and metallic tin price, can mining grade declining year by year of tin ore, current alluvial tin mining grade is reduced to 0.009% ~ 0.03%, and minimum only 0.005%, and lode tin ore deposit mining grade is about 0.5%.
Through ore-dressing technique process all the year round, what domestic each large dressing-works was accumulative reaches more than 500,000,000 tons containing tailing total amount, and is increasing with the speed of annual more than 1,000 ten thousand tons.Containing the average grade of tailing tin 0.1% ~ 0.2%, the total amount of amounting to rear metallic tin reaches more than 700,000 tons.It is reported, only the tailing that contains of Yunnan Yun Xi company just reaches 2.4 hundred million tons, and its tin grade is about 0.18%, and average Iron grade is higher than 30%.
The domestic and international recoverying and utilizing method about cassiterite mineral mainly contains gravity treatment, flotation and fuming volatilization method (comprising sulfiding volatilization, chloridizing volatilization and reduction volatilization) at present.
Gravity treatment mainly utilizes the characteristic that cassiterite density ratio intergrowth gangue mineral are large, and its production cost is low, and environmental pollution is little, is one of main method of producing cassiterite concentrate both at home and abroad, and current world tin output has more than 85% from gravity concentration.But because alluvial tin is containing a large amount of subparticle sludge, graded desliming is preparation work necessary in cassiterite reuse adoption process, this operation needs the selected grade of strict control, gets rid of the interference of sludge as far as possible.But sorting of tin ore generally adopt multistage grinding, sort the technical process that combines due to cassiterite fragility comparatively large, in grinding process, cassiterite is very easily crossed and is pulverized, and microfine is dropped with mine tailing, causes the greatly wasting of resources.
Flotation is thin for disseminated grain size, multiple valuable element association complicated ore, after ore grinding to monomer dissociation, and can the cassiterite of efficient recovery microfine.But along with higher-grade Tin Resources is day by day exhausted, floatation process needs poor, thin, the assorted degree of ore to be processed more and more higher, flotation difficulty is increasing, and the flotation of cassiterite is often needed simultaneously to other valuable metal element considering to reclaim association, thus floatation process faces the practical problemss such as subparticle content is many, pH values of pulp, regime of agent, increase flotation difficulty, reduce product recovery rate, cause the comprehensive recovery of tin how even lower below 30%, the tin still containing 0.1% ~ 0.2% in Flotation of Cassiterite milltailings does not obtain efficient recovery.Therefore, single flotation process can not meet the needs that low-grade tin ore reclaims.
Sulfuration and chlorination fuming volatilization process low-grade stanniferous iron resources comparatively effective means at present, and can realize tin iron preferably and be separated, its cardinal principle utilizes SnS and SnCl
2at high temperature volatile characteristic, mixed with reductive agent, vulcanizing agent or chlorizating agent by stanniferous material under being placed on high temperature and carry out roasting, in roasting process, tin enters gas phase with stannous compound form, and cooling in tail gas is also reclaimed at flue dust.The tin rate of recovery of fuming volatilization method is higher, but it is high to there is maturing temperature, and roasting time is long, and forms SO in roasting process
2and Cl
2deng toxic and harmful, also there is corrosion to equipment in not only contaminate environment.Above defect seriously limits the commercial introduction application of fuming volatilization technique.Patent " a kind of from ore dressing containing Separation and Recovery tin tailing method (patent No.: 201210453731.2) " adopt the reluctant stanniferous milltailings of the method process of weak reducing roasting tradition ore-dressing technique, make to reach more than 70% containing the evaporation rate of tin in tailing.Its know-why is: under hot conditions, utilizes SnO
2more easily be reduced to SnO, and the vapour pressure of SnO is large, thus realizes volatilization and the recovery of SnO.But the method does not relate to the recovery of ferro element in mine tailing, and the rate of recovery of tin is still not high.According to thermomechanical analysis, the volumetric concentration [CO/ (CO+CO of CO in the method calcination atmosphere
2)] be 20% ~ 50%, under this reducing atmosphere condition, high price ferriferous oxide is easily reduced to Fu Shi body, is unfavorable for recovery and the utilization of follow-up ferro element.
In sum, existing ore-dressing technique is adopted to be difficult to the tin iron resources realizing high efficiency separation and reclaim symbiotic relationship complexity, the tin rate of recovery of gained is low, in iron ore concentrate, Theil indices exceedes the requirement (requiring that Sn content is lower than 0.08%) of blast-furnace smelting raw material, and fuming volatilization technique exists, and energy consumption is high, cost is high, pollute the shortcomings such as large.Therefore, exploiting economy utilizes Iron Ore Containing Tin resource efficiently, and especially the difficulty of rich reserves selects the processing method of stanniferous iron tailings resource, effectively can alleviate China's tin resource and iron ore deposit situation in short supply.
Summary of the invention
, high in cost of production a series of defect low for the separation efficiency processing the existence of tin iron tailings technique in prior art, the object of the invention is to be to provide one with tin iron tailings for raw material, iron tin high efficiency separation in tin iron tailings can be realized, pollute little, the method that cost is low, the method achieve the comprehensive utilization of the resource degree of depth, meet demand of industrial production.
The invention provides a kind of method of stanniferous iron tailings separated in synchronization tin and iron, the method comprises the following steps:
Step (1): raw material agglomeration
After by stanniferous iron tailings, 100:7 ~ 10 mix in mass ratio with composite additive, by mixture agglomeration; Described composite additive is made up of following mass percent component: sodium sulfate 10% ~ 20%, borax 50% ~ 70%, SODLUM FULVATE 20% ~ 30%;
Step (2): oxidizing roasting
Step (1) gained agglomerate, after predrying, is placed in oxidizing atmosphere, carries out oxidizing roasting, obtain oxidizing roasting agglomerate at 800 DEG C ~ 900 DEG C temperature; Described oxidizing atmosphere is by O
2and N
2mixing composition, O in oxidizing atmosphere
2volume percent mark [O
2/ (O
2+ N
2)] × 100%>=10%;
Step (3): magnetizing roasting
Step (2) gained oxidizing roasting agglomerate is placed in reducing atmosphere, at 550 DEG C ~ 750 DEG C temperature, carries out reducing roasting, after reducing roasting completes, cool in an inert atmosphere, obtain reducing roasting product; Described reducing atmosphere is by CO and CO
2mixing composition, in reducing atmosphere, the volume percent fractal dimension of CO is held in 5%≤[CO/ (CO+CO
2)] × 100%≤25%;
Step (4): mill ore magnetic selection
After the reducing roasting product that step (3) obtains is milled, be separated by magnetic separation and obtain magnetite concentrate and rich tailing.
The method of separated in synchronization tin and iron from stanniferous iron tailings of the present invention also comprises following preferred version:
In preferred scheme, the oxidizing roasting time is 35min ~ 65min.
In preferred scheme, the reducing roasting time is 25min ~ 65min.
Reducing roasting product in preferred scheme in step (4) is milled until granularity mass percentage content >=80% shared by-0.074mm.
In preferred scheme, magnetic separation is separated in step (4) is be realize in the magnetic field of 800Gs ~ 1500Gs in magneticstrength.
Magnetite concentrate Iron grade >=60% of step (4) gained in preferred scheme, Theil indices < 0.08%; Tin grade > 1% in the rich tailing of gained.
Described agglomeration method comprises pelletizing or pressure group.
Innovation of the present invention is: first, and the thing that the present invention is directed to tin in stanniferous iron tailings has carried out large quantifier elimination mutually, finds that the existence of non-cassiterite state tin adopts beneficiating method Separation and Recovery to contain the major reason that in tinner skill, the tin rate of recovery is low.Existing ore-dressing technique generally for be cassiterite (SnO
2) mineral, the recovery for non-cassiterite state tin thing phase is not almost considered, and thus this type of tin mineral obtains enrichment in mine tailing.In the stanniferous iron tailings of part, the tin of non-cassiterite state accounts for the mass percentage of total tin even higher than 50%.The further lot of experiments of contriver finds, the testing sulphide of the tin mineral of non-cassiterite state mainly varlamoffite and tin, can occur to decompose or oxidizing reaction, finally form tindioxide under oxidizing roasting condition.The roasting process of contriver to stanniferous iron tailings has done a large amount of experimental studies simultaneously, find that the composite additive be made up of by a certain percentage borax, sodium sulfate and SODLUM FULVATE is under oxidizing roasting, magnetizing roasting condition, contribute to the separation strengthening tin, iron, and in dry and roasting process, agglomerate can ensure good shape, does not substantially produce powder.Therefore, the present invention finally determines to be separated with oxidizing roasting, magnetizing roasting and magnetic separation the scheme combined, can realize being that tindioxide to enter in magnetic tailing while enrichment by cassiterite state tin thing inversion of phases non-in mine tailing, and the high price reduction of ferrous oxide in original debris is become magnetite, then be separated acquisition magnetite concentrate by ore grinding, magnetic separation.
Compared with prior art, the invention has the beneficial effects as follows: the iron recovery of magnetic separation of iron ore concentrate can be made to reach more than 80%, and wherein tin residual quantity is lower than 0.08%, meets the requirement of blast furnace ironmaking raw material; Tin is mainly enriched in mine tailing with tindioxide form, and the existing beneficiation method for cassiterite mineral can be adopted to carry out being separated and reclaiming.The present invention is compared with existing method, and the present invention also has the advantages such as maturing temperature is low, the time is short, tin iron separating effect is remarkable, be specially adapted to process tin iron symbiotic relationship closely, adopt existing beneficiation method to be difficult to the stanniferous iron tailings of Separation and Recovery.Adopt technology provided by the present invention, can iron in high efficiency separation tin iron tailings and tin, thus realize the difficult comprehensive reutilization of stanniferous iron tailings that selects and process with increment.
Accompanying drawing explanation
[Fig. 1] is process flow sheet of the present invention.
Embodiment
Following examples are intended to further illustrate this content of the present invention, instead of restriction scope.
Comparative example 1
Do not add complex additive of the present invention in this comparative example, do not carry out oxidizing roasting yet:
First stanniferous iron tailings (tin grade 0.45%, Iron grade 40.21%) is dehydrated and carry out agglomeration to certain moisture, dry; Dried agglomerate is put into stoving oven, roasting under the maturing temperature of 600 DEG C, pass into the volumetric concentration [CO/ (CO+CO of CO in reducing gas
2)] × 100% be 15%, roasting time 65min, after roasting terminates, by roasting agglomerate at N
2under atmosphere after cooling, levigately be less than 0.074mm to 80%, magnetic separation under magneticstrength is 1000Gs condition, obtain the iron ore concentrate (wherein the grade 0.32% of tin) of Iron grade 61.12%, iron recovery 80.21%, obtains the grade 0.55% (wherein the tin of 66.3% exists with tindioxide) of tin in rich tailing.Tin iron inferior separating effect, magnetic separation obtains the stanniferous grade of iron ore concentrate far above 0.08%, can not directly use as blast furnace burden.
Comparative example 2
With the addition of complex additive of the present invention in this comparative example, but do not carry out oxidizing roasting:
First by stanniferous iron tailings (tin grade 0.83%, Iron grade 34.21%) dehydrate to certain moisture, with addition of the composite additive (mass ratio of different components is sodium sulfate: borax: SODLUM FULVATE=10%:70%:20%) accounting for mine tailing (butt) mass percent 7%, after mixing of materials is even, agglomeration, dry; Dried agglomerate is put into stoving oven, roasting under the maturing temperature of 550 DEG C, pass into the volumetric concentration [CO/ (CO+CO of CO in reducing gas
2)] × 100% be 25%, roasting time 65min, after roasting terminates, by roasting agglomerate at N
2under atmosphere after cooling, levigately be less than 0.074mm to 80%, magnetic separation under magneticstrength is 800Gs condition, obtain the iron ore concentrate (wherein the grade 0.33% of tin) of Iron grade 60.23%, iron recovery 81.14%, obtains the grade 1.02% (tin of 79.9% exists with tindioxide) of tin in rich tailing.Tin iron inferior separating effect, magnetic separation obtains the stanniferous grade of iron ore concentrate far above 0.08%, can not directly use as blast furnace burden.
Embodiment 1
First by stanniferous iron tailings (tin grade 0.55%, Iron grade 40.21%) dehydrate to certain moisture, with addition of the composite additive (mass ratio of different components is sodium sulfate: borax: SODLUM FULVATE=10%:70%:20%) accounting for mine tailing (butt) mass percent 10%, after mixing of materials is even, agglomeration, dry; Dried agglomerate is put into stoving oven, passes into nitrogen protection, be warming up to 900 DEG C, after treating temperature-stable, pass into O
2volumetric concentration [O
2/ (O
2+ N
2)] × 100% be 10% mixed gas roasting 35min, then be cooled to 750 DEG C, pass into the volumetric concentration [CO/ (CO+CO of CO in reducing gas
2)] × 100% be 5%, roasting time 25min, after roasting terminates, by roasting agglomerate at N
2under atmosphere after cooling, be levigately less than 0.074mm, magnetic separation under magneticstrength is 1000Gs condition to 80%.Obtain the magnetite concentrate (wherein the grade 0.05% of tin) of Iron grade 64.31%, iron recovery 83.11%, obtain the grade 1.12% (wherein the tin of 94.1% exists with tindioxide) of tin in rich tailing.
Embodiment 2
First by stanniferous iron tailings (tin grade 0.83%, Iron grade 34.21%) dehydrate to certain moisture, with addition of the composite additive (mass ratio of different components is sodium sulfate: borax: SODLUM FULVATE=20%:50%:30%) accounting for mine tailing (butt) mass percent 7%, after mixing of materials is even, agglomeration, dry; Dried agglomerate is put into stoving oven, passes into nitrogen protection, be warming up to 850 DEG C, after treating temperature-stable, pass into O
2volumetric concentration [O
2/ (O
2+ N
2)] × 100% be 21% mixed gas roasting 40min, then be cooled to 550 DEG C, pass into the volumetric concentration [CO/ (CO+CO of CO in reducing gas
2)] × 100% be 25%, roasting time 65min, after roasting terminates, by roasting agglomerate at N
2under atmosphere after cooling, levigately be less than 0.074mm to 80%, magnetic separation under magneticstrength is 800Gs condition, obtain the iron ore concentrate (wherein the grade 0.07% of tin) of Iron grade 62.34%, iron recovery 84.22%, obtains the grade 1.66% (wherein the tin of 94.3% exists with tindioxide) of tin in rich tailing.
Embodiment 3
First by stanniferous iron tailings (tin grade 1.13%, Iron grade 42.24%) dehydrate to certain moisture, with addition of the composite additive (mass ratio of different components is sodium sulfate: borax: SODLUM FULVATE=15%:63%:22%) accounting for mine tailing (butt) mass percent 8%, after mixing of materials is even, agglomeration, dry; Dried agglomerate is put into stoving oven, passes into nitrogen protection, be warming up to 800 DEG C, after treating temperature-stable, pass into O
2volumetric concentration [O
2/ (O
2+ N
2)] × 100% be 40% mixed gas roasting 65min, then be cooled to 700 DEG C, pass into the volumetric concentration [CO/ (CO+CO of CO in reducing gas
2)] × 100% be 10%, roasting time 55min, after roasting terminates, by roasting agglomerate at N
2under atmosphere after cooling, be levigately less than 0.074mm, magnetic separation under magneticstrength is 1500Gs condition to 80%.Obtain the iron ore concentrate (wherein the grade 0.05% of tin) of Iron grade 60.34%, iron recovery 85.34%, obtain the grade 2.01% (wherein the tin of 96.5% exists with tindioxide) of tin in rich tailing.
Embodiment 4
First by stanniferous iron tailings (tin grade 1.02%, Iron grade 26.43%) dehydrate to certain moisture, with addition of the composite additive (mass ratio of different components is sodium sulfate: borax: SODLUM FULVATE=17%:60%:23%) accounting for mine tailing (butt) mass percent 9%, after mixing of materials is even, agglomeration, dry; Dried agglomerate is put into stoving oven, passes into nitrogen protection, be warming up to 830 DEG C, after treating temperature-stable, pass into O
2volumetric concentration [O
2/ (O
2+ N
2)] × 100% be 55% mixed gas roasting 50min, then be cooled to 650 DEG C, pass into the volumetric concentration [CO/ (CO+CO of CO in reducing gas
2)] × 100% be 20%, roasting time 40min, after roasting terminates, by roasting agglomerate at N
2under atmosphere after cooling, be levigately less than 0.074mm, magnetic separation under magneticstrength is 1100Gs condition to 80%.Obtain the iron ore concentrate (tin grade 0.07%) of Iron grade 60.34%, iron recovery 84.34%, obtain the grade 1.66% (wherein the tin of 95.8% exists with tindioxide) of tin in rich tailing.
Claims (6)
1. a method for stanniferous iron tailings separated in synchronization tin and iron, is characterized in that, comprise the following steps:
Step (1): raw material agglomeration
After by stanniferous iron tailings, 100:7 ~ 10 mix in mass ratio with composite additive, by mixture agglomeration; Described composite additive is made up of following mass percent component: sodium sulfate 10% ~ 20%, borax 50% ~ 70%, SODLUM FULVATE 20% ~ 30%;
Step (2): oxidizing roasting
Step (1) gained agglomerate, after predrying, is placed in oxidizing atmosphere, carries out oxidizing roasting, obtain oxidizing roasting agglomerate at 800 DEG C ~ 900 DEG C temperature; Described oxidizing atmosphere is by O
2and N
2mixing composition, O in oxidizing atmosphere
2volume percent mark [O
2/ (O
2+ N
2)] × 100%>=10%;
Step (3): magnetizing roasting
Step (2) gained oxidizing roasting agglomerate is placed in reducing atmosphere, at 550 DEG C ~ 750 DEG C temperature, carries out reducing roasting, after reducing roasting completes, cool in an inert atmosphere, obtain reducing roasting product; Described reducing atmosphere is by CO and CO
2mixing composition, in reducing atmosphere, the volume percent fractal dimension of CO is held in 5%≤[CO/ (CO+CO
2)] × 100%≤25%;
Step (4): mill ore magnetic selection
After the reducing roasting product that step (3) obtains is milled, be separated by magnetic separation and obtain magnetite concentrate and rich tailing.
2. method according to claim 1, is characterized in that, the oxidizing roasting time is 35min ~ 65min.
3. method according to claim 1, is characterized in that, the reducing roasting time is 25min ~ 65min.
4. method according to claim 1, is characterized in that, described reducing roasting product is milled until granularity mass percentage content >=80% shared by-0.074mm.
5. method according to claim 1, is characterized in that, it is be realize in the magnetic field of 800Gs ~ 1500Gs in magneticstrength that described magnetic separation is separated.
6. the method according to any one of Claims 1 to 5, is characterized in that, magnetite concentrate Iron grade >=60% of gained in step (4), the mass content < 0.08% of tin; Tin grade > 1% in the rich tailing of gained.
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Cited By (1)
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| CN112279297B (en) * | 2020-11-25 | 2022-02-11 | 中南大学 | Method for selectively separating tin from electronic waste and synchronously preparing nano tin dioxide |
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